反应详情

温度

85 °C

To a solution of 149 g (0.785 mol) of 2-acetylsulfanyl-2-methyl-propionic acid ethyl ester in EtOH (1.2 L, degassed under nitrogen for 1 h) are added 169.7 g (0.105 mol) of sodium methoxide, followed by a solution of 150 g (0.785 mol) of 4-bromo-1,1,1-trifluoro-butane. The reaction is heated to 85° C. for 3 d. The solvent is removed under reduced pressure. The residue is dissolved in DCM (1 L) and washed with saturated aq. NaHCO3 solution (2×1 L). The organic layer is dried over Na2SO4, filtered and the filtrate is concentrated under reduced pressure to afford 171 g of 2-methyl-2-(4,4,4-trifluoro-butylsulfanyl)-propionic acid ethyl ester. Yield: 84%; ESI-MS: 259 [M+H]+

1. customThe solvent is removed under reduced pressure
2. dissolutionThe residue is dissolved in DCM (1 L)
3. washwashed with saturated aq. NaHCO3 solution (2×1 L)
4. dry with materialThe organic layer is dried over Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate is concentrated under reduced pressure